EP0414182A1 - Appareil pour déterminer la vitesse de consommation biochimique de l'oxygène, et son utilisation - Google Patents

Appareil pour déterminer la vitesse de consommation biochimique de l'oxygène, et son utilisation Download PDF

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Publication number
EP0414182A1
EP0414182A1 EP90115907A EP90115907A EP0414182A1 EP 0414182 A1 EP0414182 A1 EP 0414182A1 EP 90115907 A EP90115907 A EP 90115907A EP 90115907 A EP90115907 A EP 90115907A EP 0414182 A1 EP0414182 A1 EP 0414182A1
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EP
European Patent Office
Prior art keywords
oxygen
reaction vessel
marked
absorber
determining
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP90115907A
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German (de)
English (en)
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EP0414182B1 (fr
Inventor
Wolfgang Tappe
Heinrich Dr. Keusen
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Forschungszentrum Juelich GmbH
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Forschungszentrum Juelich GmbH
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/18—Water
    • G01N33/1806—Biological oxygen demand [BOD] or chemical oxygen demand [COD]

Definitions

  • the invention relates to a device for determining the biochemical oxygen consumption rate with a reaction vessel with devices for introducing microorganisms and substrate liquid, which is connected via a CO2 absorber to an electrolytic oxygen generator and a pressure indicator, and a recording device for the reaction vessel in the blocked route - CO2 absorber - oxygen generator - pressure indicator generated oxygen quantities.
  • the biochemical oxygen consumption rate of a system of microorganisms and substrate gives an indication of the activity of the microorganisms on the one hand and (in the case of known microorganisms of known concentration) on the content of biodegradable ingredients. It is used in particular in the field of aerobic wastewater treatment to determine the activated sludge activity and the level of pollution of the wastewater to be treated.
  • the German standard procedure (DEV 1988) for determining the "oxygen consumption rate” is known as a parameter for the activity of activated sludge.
  • a synthetic waste water is added to an activated sludge sample, which is then Is ventilated for 30 minutes.
  • the decrease in the concentration of dissolved oxygen is then measured in an enclosed, bubble-free vessel using an oxygen probe.
  • the "oxygen consumption rate” is calculated from the decrease rate.
  • a measuring unit of the Sapromaten® includes a reaction vessel, an oxygen generator and a pressure indicator, which are connected to each other by plastic hoses and housed in a temperature-controlled water bath. This closed measuring system is independent of fluctuations in air pressure.
  • the sample to be examined is circulated in the reaction vessel by a magnetic stirrer, so that the amount of oxygen required to break down the waste water pollutants can penetrate into the substrate from the gas space above.
  • the gas change (O2 entry, CO2 production with subsequent CO2 absorption) creates a negative pressure, whereupon the pressure indicator responds and activates the oxygen generation up to pressure equalization via a switching amplifier.
  • the electrolysis current used for the generation of oxygen is taken as a measure of the amount of oxygen consumed by the biomass at each measurement point.
  • This device which can be used for long-term investigations, is, however, suitable for the continuous determination of the biochemical oxygen consumption rate over a short period of time, e.g. B. 1 hour less suitable:
  • the aim of the invention is therefore an improved device in this regard.
  • the device according to the invention of the type mentioned at the outset is characterized by an oxygen measuring probe in the reaction vessel for determining the dissolved oxygen in the same and a measuring and control computer connected to the measuring probe as a recording device which indicates corrected oxygen consumption rates via the temporal change in dissolved oxygen.
  • the oxygen consumption rate determined with the Sapromaten® does not correspond to the true value for short-term measurements and, in particular, high activity of the microorganisms, since the dissolved oxygen in the reaction vessel has a deficit compared to the saturation value when the pressure is equalized. For this reason, according to the invention monitors the value of the oxygen consumption rate of the dissolved oxygen in the reaction liquid, which is determined electrophotically, and takes into account its change over time as a correction element in determining the true oxygen consumption value.
  • This gas circulation reduces the O2 concentration gradient from the electrolysis cell to the reaction vessel and reduces the oxygen deficit in the reaction vessel.
  • the gas circuit also accelerates the CO2 absorption from the gas phase by continuously passing the gas stream through a CO2 absorber section, so that measurement errors due to delayed CO2 absorption are reduced.
  • soda lime is suitable for CO2 absorption, but would be useful on carbonate buffer systems (e.g. carbonate / bicarbonate mixtures).
  • a reaction vessel 1 an oxygen generator 2, a pressure measuring cell 3 and a measuring and control device 4 are provided in the device according to the invention analogous to the Sapromat ®, and a thermostat, not shown in the figure, for example by means of a water bath.
  • the reaction vessel 1 is modified from that of the Sapromaten® and typically comprises: an O2 measuring probe 5 for the continuous monitoring of the dissolved oxygen and connections 6, 7 and 8 for the supply of microorganism suspension (6), wastewater or substrate solution (7) and the gas inflow (8) of the gas circulation with gas outlet 9. Waste water / microorganism suspension are discharged via connection 10. Another connection 11 in connection with a reservoir 12 for standard nutrient solution with shut-off valve 13 is used to determine the presence of inhibitors given below.
  • reaction vessel is cylindrical and has e.g. B. a volume of 300 ml.
  • the O2 measuring probe is introduced gas-tight over flanges.
  • a further implementation can be provided for a pH measuring probe.
  • the filling and emptying is preferably carried out centrally controlled by appropriate pumps.
  • FIG. 1 shows feed pumps 16, 17, 18 (e.g. peristaltic pumps with a delivery rate of about 200 ml / min, computer-controlled delivery time or amount) for the supply of microorganisms, waste water and nutrient solution and 19 for the removal of microorganisms / Waste water from the reaction vessel 1.
  • a waste water storage container (of, for example, 70 ml) with a shut-off valve 20 '(for example a solenoid valve) is designated by 20.
  • the container 20 is included in the gas circuit, so that from 20 pressure-free in the closed system waste water (over 17) or standard nutrient solution (over 18 with associated storage vessel 12 ') can be filled into the reaction vessel 1.
  • a directly connected storage vessel 12 for standard nutrient solution can also be provided, as indicated in FIG. 2, which is then integrated into the gas circuit for ventilation.
  • 21 is a computer-controlled pressure compensation valve and 22, 22 'is a computer-controlled magnetic stirrer for vessel 1 (with a constant, adjustable speed of, for example, 150, 200, 250 rpm or electronic speed control).
  • the central measurement and control computer 23 e.g. a hybrid recorder from Chessell
  • BSR biochemical oxygen consumption rate
  • the storage container 20 is filled with waste water and / or nutrient solution and the reaction vessel 1 is filled with the microorganism suspension.
  • the pressure compensation valve 21 is open and the shut-off valve of the reservoir 20 'is closed.
  • the liquid volumes can be freely selected depending on the requirements, only the sum of both volumes must be known. It is included in the conversion of the volume-related, electrolytically produced oxygen (BSV).
  • the measuring and control unit 4 calculates the BSV on the basis of 250 ml sample volume. (With the corresponding programming of 23, 4 can be omitted.) If the sample volume Vx deviates from the nominal volume Vo, the measured values must be multiplied by the factor Vx / Vo.
  • the pressure compensation valve 21 is closed.
  • the sample is stirred for at least 5 minutes for the purpose of temperature adjustment and adjustment of the CO2 / O2 equilibrium.
  • the stirring speed is set to an empirically determined value of e.g. B. 150 rpm.
  • the control and computing unit 23 continuously records the O2 and BSV values and calculates the BSR values.
  • the stirring speed is adjusted so that the O2 concentration at a rate of z. B. 1 mg O2 / (1 x min) increases. Once a threshold of e.g. B. 6 mg / l is reached, the stirring speed is set to the current value.
  • the adjustment phase is ended after the specified period of time (for example 5 minutes) or if a period of e.g. B. one minute the O2 and BSR values show constant values (+/- 10% of the mean). If both conditions are met, the shut-off valve 20 'opens and releases the liquid into the reaction vessel 1. Typically, the O2 concentration drops to ⁇ 5 mg O2 / l after the liquid has been added. If the value falls below 1 mg / l, the stirring speed should be increased (e.g. gradually by 20% each time) to avoid an undersupply of oxygen. If O2 minima of> 5 mg / l are measured, the stirring speed can be reduced if necessary (e.g. 20%). This is particularly necessary if the electrolytic cell 2 is used for a long time room (> 2 min) permanently produces O2. This is to be avoided as it leads to a minor round.
  • the measurement is completed after a defined period of time (e.g. 1 h) or after the activity has dropped below a setpoint.
  • a 10-minute period can be defined as the target value in which BSR values are measured which are at most 10% above the BSR values measured before substrate addition.
  • the pressure compensation valve is opened. Depending on the requirements, a new wastewater surge is conveyed into the storage container (shut-off valve closed) and the measurement is repeated with the same microorganism suspension. Otherwise, the total wastewater / microorganism mixture is conveyed out of the sample vessel.
  • FIG. 3 A simple laboratory variant of the device described above is shown in FIG. 3. Contrary to the automatic filling and emptying of the reaction vessel described in FIG. 1 by means of controllable shut-off valves and pumps, these processes take place manually. Measuring principle, reaction vessel and CO2 absorption correspond to Fig. 1.
  • the reaction vessel 1 is mixed by means of a magnetic stirrer 22.
  • the pressure indicator 3 triggers the oxygen production by the oxygen generator 2 when the pressure drops.
  • the amount of oxygen produced is recorded by the registration device 24 and continuously fed to the computer 25.
  • the oxygen electrode 5 located in the reaction vessel 1 feeds the computer 25, via the measuring amplifier 26, the current oxygen concentration in the sample solution, the change in time of which represents the correction element when determining the true oxygen consumption value.
  • the device described is particularly suitable for controlling the substrate supply in biotechnological processes as a function of the oxygen consumption.
  • the serial measurement of the activity of the test organisms after addition of a nutrient solution and the subsequent investigation of a mixture of nutrient solution and waste water containing inhibitor are provided.
  • the nutrient solution is conveyed into the storage container in the first measuring phase and the activity of the microorganisms is examined after the nutrient solution has been added (“normal activity”).
  • the Nutrient solution After completion of the first measurement phase, the Nutrient solution, the inhibitor-containing wastewater is pumped into the storage container and the measurement is repeated.
  • the measured values of the second measurement phase are compared with the values of the first phase. In the presence of inhibitors in the wastewater, the expected value after the addition of wastewater is not reached, from which the inhibitory effect can be concluded.
  • Nitrifiers react particularly sensitively when testing inhibitors.
  • FIG. 4 and FIG. 5 A typical course of such BSR curves is shown in FIG. 4 and FIG. 5, which were obtained using activated sludge samples fed with model waste water:
  • the values measured before the addition of substrate (S) correspond to the basic oxygen consumption of the "starved” activated sludge. After substrate addition, the oxygen consumption rate increases and returns to the basic rate after a period of approx. 30 minutes (consumption phase). These values did not change during the subsequent "hunger phase".
  • the area below the curve during the feeding phase is characteristic of the wastewater load and the current activity of the microorganisms.
  • FIG. 5 shows an example of the influence of an inhibitor (dimethyl disulfide) on breathability.
  • the nitrificants in particular react sensitively to this inhibitor.
  • the ammonium contained in the model wastewater is no longer oxidized due to inhibited nitrification in the same way as in the experiment shown in FIG. 4 (no "nitrification plateau").

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EP19900115907 1989-08-23 1990-08-20 Appareil pour déterminer la vitesse de consommation biochimique de l'oxygène, et son utilisation Expired - Lifetime EP0414182B1 (fr)

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DE8910097U DE8910097U1 (de) 1989-08-23 1989-08-23 Vorrichtung zur Bestimmung der biochemischen Sauerstoffverbrauchsrate
DE8910097U 1989-08-23

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EP0414182A1 true EP0414182A1 (fr) 1991-02-27
EP0414182B1 EP0414182B1 (fr) 1994-07-13

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4300575A1 (de) * 1993-01-12 1994-07-14 Alois Hoerl Verfahren und Messanordnung zur Ermittlung biologisch wirksamer Einflüsse auf biologische Zellsysteme
EP0642011A1 (fr) * 1992-07-30 1995-03-08 J.M. Voith GmbH Appareil pour déterminer le besoin en oxygène
DE4340098A1 (de) * 1993-11-25 1995-06-01 Koop Winfried Dr Agr Vorrichtung zur Messung des Indikators der mikrobiellen Biomasse nach der Methode der Substrat-induzierten Atmung (SIR)
DE4423848A1 (de) * 1994-07-07 1996-01-11 Wtw Weilheim Integriertes Analysengerät zur Bestimmung des Gasverbrauchs von Materie
DE19609071A1 (de) * 1996-03-08 1997-09-11 Wtw Weilheim Verfahren zur Fehlervermeidung bei der Messung oder Bestimmung des Gasverbrauchs von Materie
WO2000011464A1 (fr) * 1998-08-18 2000-03-02 Biochem Technology, Inc. APPAREIL ET PROCEDE DE MESURE DU NOx ET DU TAUX DE NITRIFICATION/DENITRIFICATION DANS DES PROCESSUS BIOCHIMIQUES
NL1026287C2 (nl) * 2004-05-28 2005-11-30 Vitens Fryslsn Werkwijze en inrichting voor het bepalen van de microbiologische activiteit van een waterige oplossing.
US7449113B2 (en) 2002-09-24 2008-11-11 Advanced Aeration Control, Llc Controlling wastewater treatment processes
RU2510021C2 (ru) * 2012-01-31 2014-03-20 Федеральное государственное бюджетное учреждение науки Институт водных проблем Российской академии наук (ИВП РАН) Способ и устройство для непрерывного измерения биохимического потребления кислорода, биохимической потребности в кислороде и скорости биохимического окисления
RU2608443C2 (ru) * 2015-05-28 2017-01-18 ООО "НПФ "Альфа БАССЕНС" Способ экспресс-анализа биохимического потребления кислорода и устройство для его осуществления

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE502005004458D1 (de) 2005-07-16 2008-07-31 Pauly Udo Verfahren zur Bestimmung der metabolischen Stabilität von Schlamm, insbesondere von Klärschlamm

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2163612A1 (de) * 1971-12-21 1973-06-28 Passavant Werke Verfahren und vorrichtung zum messen und/oder ueberwachen des gehaltes an biologisch abbaubarer organischer materie in einer probenfluessigkeit
US3810738A (en) * 1972-08-14 1974-05-14 L Fleischmann Bod measuring apparatus
FR2418201A1 (fr) * 1978-02-23 1979-09-21 Voith Gmbh Procede et dispositif de mesure de la demande biologique en oxygene
DE2952343A1 (de) * 1979-12-24 1981-06-25 Linde Ag, 6200 Wiesbaden Verfahren und vorrichtung zur bestimmung des sauerstoffverbrauchs in belebungsbecken
DE3128439A1 (de) * 1981-07-18 1983-02-03 Boehringer Mannheim Gmbh, 6800 Mannheim Verfahren und vorrichtung zur bestimmung von abwasserparametern
FR2598834A1 (fr) * 1986-05-16 1987-11-20 Univ Alberta Procede et appareil destines a apporter une amelioration a la determination de la vitesse d'absorption de l'oxygene dans les stations de traitement d'eaux usees

Family Cites Families (5)

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FR2016328A1 (en) * 1968-08-24 1970-05-08 Comitato Nale En Nu Measurement of biochemical oxygen demand - istry
US4073692A (en) * 1975-04-21 1978-02-14 Ciaccio Leonard L Method and apparatus for automated measurement of energy oxygen
DE3118651A1 (de) * 1981-05-11 1982-12-02 Jürgen 5060 Bergisch-Gladbach Hamann Verfahren zur bestimmung der keimzahl in mit aeroben mikroorganismen kontaminierten proben
JPS60217837A (ja) * 1984-04-13 1985-10-31 エンジニヤリング・アンド・リサーチ・アソシエーツ・インコーポレーテツド 小宇宙およびその構成方法
DE3626231A1 (de) * 1986-08-02 1988-03-03 Gerhard Velebil Fluessigkeits-gas-dispersionsreaktor

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2163612A1 (de) * 1971-12-21 1973-06-28 Passavant Werke Verfahren und vorrichtung zum messen und/oder ueberwachen des gehaltes an biologisch abbaubarer organischer materie in einer probenfluessigkeit
US3810738A (en) * 1972-08-14 1974-05-14 L Fleischmann Bod measuring apparatus
FR2418201A1 (fr) * 1978-02-23 1979-09-21 Voith Gmbh Procede et dispositif de mesure de la demande biologique en oxygene
DE2952343A1 (de) * 1979-12-24 1981-06-25 Linde Ag, 6200 Wiesbaden Verfahren und vorrichtung zur bestimmung des sauerstoffverbrauchs in belebungsbecken
DE3128439A1 (de) * 1981-07-18 1983-02-03 Boehringer Mannheim Gmbh, 6800 Mannheim Verfahren und vorrichtung zur bestimmung von abwasserparametern
FR2598834A1 (fr) * 1986-05-16 1987-11-20 Univ Alberta Procede et appareil destines a apporter une amelioration a la determination de la vitesse d'absorption de l'oxygene dans les stations de traitement d'eaux usees

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0642011A1 (fr) * 1992-07-30 1995-03-08 J.M. Voith GmbH Appareil pour déterminer le besoin en oxygène
DE4300575A1 (de) * 1993-01-12 1994-07-14 Alois Hoerl Verfahren und Messanordnung zur Ermittlung biologisch wirksamer Einflüsse auf biologische Zellsysteme
DE4340098A1 (de) * 1993-11-25 1995-06-01 Koop Winfried Dr Agr Vorrichtung zur Messung des Indikators der mikrobiellen Biomasse nach der Methode der Substrat-induzierten Atmung (SIR)
DE4423848C2 (de) * 1994-07-07 1999-01-28 Wtw Weilheim Analysengerät zur Bestimmung des biochemischen Sauerstoffbedarfs von Materie
DE4423848A1 (de) * 1994-07-07 1996-01-11 Wtw Weilheim Integriertes Analysengerät zur Bestimmung des Gasverbrauchs von Materie
DE19609071C2 (de) * 1996-03-08 2000-05-18 Wtw Weilheim Verfahren zur Fehlervermeidung bei der Messung oder Bestimmung des Gasverbrauchs von Materie
US5929317A (en) * 1996-03-08 1999-07-27 Wtw Wissenschaftlich-Technische Wekkstatten Gmbh Process for avoiding error in measuring or determining the gas consumption of matter
DE19609071A1 (de) * 1996-03-08 1997-09-11 Wtw Weilheim Verfahren zur Fehlervermeidung bei der Messung oder Bestimmung des Gasverbrauchs von Materie
EP0794431A3 (fr) * 1996-03-08 2000-11-22 WTW Wissenschaftlich-Technische Werkstätten GmbH Méthode pour éviter des erreurs pendant la mesure ou la détermination de la consommation de gaz par une matière
WO2000011464A1 (fr) * 1998-08-18 2000-03-02 Biochem Technology, Inc. APPAREIL ET PROCEDE DE MESURE DU NOx ET DU TAUX DE NITRIFICATION/DENITRIFICATION DANS DES PROCESSUS BIOCHIMIQUES
US6143246A (en) * 1998-08-18 2000-11-07 Biochem Technology, Inc. Apparatus for measuring ammonia in biochemical processes
US6416652B1 (en) 1998-08-18 2002-07-09 Bio Chem Technology, Inc. Method for measuring ammonia in biochemical processes
RU2228523C2 (ru) * 1998-08-18 2004-05-10 БАЙОКЕМ ТЕКНОЛОДЖИ, Инк. Способы измерения скоростей нитрификации и денитрификации и nox в жидкости
US7449113B2 (en) 2002-09-24 2008-11-11 Advanced Aeration Control, Llc Controlling wastewater treatment processes
NL1026287C2 (nl) * 2004-05-28 2005-11-30 Vitens Fryslsn Werkwijze en inrichting voor het bepalen van de microbiologische activiteit van een waterige oplossing.
RU2510021C2 (ru) * 2012-01-31 2014-03-20 Федеральное государственное бюджетное учреждение науки Институт водных проблем Российской академии наук (ИВП РАН) Способ и устройство для непрерывного измерения биохимического потребления кислорода, биохимической потребности в кислороде и скорости биохимического окисления
RU2608443C2 (ru) * 2015-05-28 2017-01-18 ООО "НПФ "Альфа БАССЕНС" Способ экспресс-анализа биохимического потребления кислорода и устройство для его осуществления

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EP0414182B1 (fr) 1994-07-13
DE8910097U1 (de) 1989-10-05
DE59006412D1 (de) 1994-08-18

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